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Engineering research paper

International Journal of Engineering and Technical Research (IJETR)

ISSN: 2321-0869, Volume-3, Issue-4, April 2015

Influence of process parameters on Electrodeposited

Nickel thin film coating using Taguchi approach

S.Jeyaraj, G.Muralidharan, K.P.Arulshri, R.Saravanan

microstructures. Nickel plating is very important for a

microelectromechanical systems (MEMS) device with a

better electrical and thermal conductivity and also important

for applications like small integrated systems with sensors,

signal conditioning circuits, actuators and with special

functions with a size of few micrometers [1].

Abstract—In this study, Nickel thin film coatings were

prepared from watts bath with the aid of electrodepostion

process over a mild steel substrate. The process parameters

current density, pH, bath temperature and time of deposition

were considered for experimental work. The L27 orthogonal

array of taguchi design was chosen for experimental design.

Based on the run orders of experimental design the experiments

were conducted. Micro hardness of thin film coatings were

examined in Vickers micro hardness tester under the pay load of

50 gram force. The surface morphologies of coatings were

investigated with scanning electron microscopic analysis and the

deposition of nickel were confirmed by EDX analysis. The

influences of process parameters on micro hardness of nickel

coatings were investigated with S/N ratio analysis and mean

effects studies via Taguchi approach and parameters were

ranked by order. It is observed that current density and time of

deposition were most influencing factor for micro hardness of

Nickel coating. In order to confirm the rank positions, Analysis

of variances (ANOVA) test were conducted and resulted the

similar rank positions of S/N ratio and mean effects studies.

Zhao et al [2] had developed a nickel thin film in

sulphamate bath at different current densities ranging from

0.01 A/cm2 to 0.1 A/cm2. They investigated the

microstructure and corrosion behaviors of electrodeposited

nickel developed at different current densities. It was

indentified that during electrodeposition grain size increased

with increasing current density, the dense surface

microstructure of electrodeposited nickel was developed at

0.05A/cm2. The prepared nickel samples possessed

with active–passive–trans passive polarization properties.

Better corrosion resistance in nickel plating was obtained at

0.05 A/cm2 of current density.

nickel coating onto AZ91 Mg alloy. They concluded that

depositing a pore-free nickel coating with average grain size

of 95 nm can be accomplished by using proper initiation,

zincating and Cu electrode-position pretreatment processes.

The nickel layer developed in this condition can efficiently

improve the corrosion resistance and hardness of AZ91 Mg

alloy that makes it more dependable for industrial

applications. Zengwei Zhu [4] had prepared bright nickel

electro deposited coating under perturbation of hard particles.

They found that bright nickel deposit was FCC structure. The

surface roughness was about 0.016 μm and the grain size was

less than 80 nm.

Arman zarebidaki [3] had prepared electrodeposited

Index Terms— ANOVA; Electro deposition; micro

hardness; S/N ratio

I.INTRODUCTION

Electrodeposition has been acknowledged as a feasible and

cost effective technique for producing of thin film coating.

Electrodeposited materials are possessed with optimal

mechanical properties and suitable for fabrication of

micromechanical components with better properties than that

of conventional type fabrication. Numerous metals or alloys

can be electroplated with different properties can be attained.

Electroplating is well-suited with integrated circuits

production as it is low-temperature and high rate deposition

technology.

must be carefully assessed before discussing the influence of

their microstructure on properties [5]. ZHOU Li-qu et al [6]

had equipped the forming limits of nickel coating. They

concluded that the forming limit of the nickel coating is not as

good as that of the steel substrate, and the forming limited

strain of the coating sheet tends to moderate with the rise of

thickness of the coating.

Chemical contamination of electrodeposited coatings

Nickel is an extensively applied material for thin film

coating by electrodeposition. The nickel thin film coatings

were prepared by different grain structures by above process.

Large grained Ni coating is anticipated to distort easier

whereas fine-grained structured electrodeposited nickel will

resist the deformation. Electrodeposited nickel possessed

with good mechanical properties such as high yield strength

and hardness that are advantageous with the elevated

Nickel coating on Al 2014 alloy. This experimental result

indicates that electrochemical deposition combined with heat

treatment can be used to improve the surface properties of Al

alloy. Anette A. Rasmussen [8] concluded that the current

density and the temperature only have a limited effect on the

microstructure and the hardness.

A- Ul-Hamid et al [7] had prepared electro deposited

Manuscript received March 30, 2015.

S.Jeyaraj, Assistant Professor, School of MechanicalEngineering,

SASTRA University, Tamil nadu , India.

G.Muralidharan, PG scholar, School of Mechanical Engineering,

SASTRA University, Tamil nadu, India.

K.P. Arulshri, Professor and Head, department of Mechatronics,

Bannari Amman Institute of technology, Tamil nadu, India.

R.Saravanan, PG scholar, School of Mechanical Engineering,

SASTRA University, Tamil nadu, India.

Suman and sahoo [9] had prepared the electroless Ni-B

composite coating and investigated the influences of process

parameters on microharness of coating with the help of

taguchi analysis. They took four parameters; temperature of

bath, nickel source concentration, concentration of reducing

agent and annealing temperature, and framed into an L27

1 www.erpublication.org


Engineering research paper

Influence of process parameters on Electrodeposited Nickel thin film coating using Taguchi approach

III.MATERIALSANDMETHODS

Electrocodeposition experiments were conducted in

a 1000 ml glass beaker. The electrolyte used for plating work

was a watts type nickel bath. Mild steel plate of sized 70 ×

25.4 × 1 mm3 was used as a cathode substrate and area of

deposition taken as 25.4× 25.4mm3 (1 inch2). The left behind

portions of plating area were masked. A pure nickel plate was

used as anode. A Nickel anode plate of sized 95× 35 × 8 mm3

thick was employed in the circuit. The mild steel cathode

plate was degreased by acetone and polished with dry cloth

buffing wheel, for exclusion of rust layer. The distance

between Ni anode and mild steel cathode was engaged

constantly [14]. A regulated power supply unit made by

Spark Tek (0-2A, 0 – 30V, DC supply) was used for the

electroplating. The bath temperature was accurately

controlled using K-type thermocouple. The pH of the solution

was monitored by digital pH meter. The pH of bath was

attuned with diluted H2SO4 and NaOH solutions depending

upon the plating conditions. The plating conditions taken for

these experimental tests are given in table I. The experiments

were performed based on the run orders of L27 orthogonal

array pattern and twenty seven samples were prepared from

the bath.

orthogonal array to determine the significances of process

parameters on hardness of the coating with the help of

analysis of variance, which exposed that annealing

temperature and concentration of reducing agent have

significant influence on hardness characteristics of electroless

Ni-B coating. With the above illustrations, statistical

prediction models have applied in various field investigations

to evaluate the best levels of the process parameters by many

researchers [10-12].

However, previous experimental studies in electro

deposition were accomplished by randomized manner. Only

few process parameters were considered in statistical studies

in identify the influences on microhardness, volume fractions

and coating thickness. Selection of process parameters also

has not been done in proper categorization. In this article,

four principal process parameters of electrodepostion process

such as current density, pH of bath, time of deposition and

bath temperature are considered on micro hardness of Ni thin

film coatings. The taguchi method of L27 orthogonal array

has been employed to study the influences of process

parameters on microhardness of Ni thin film coating. With

these, Analysis of Variance (ANOVA) techniques has been

applied to determine the significance of these parameters.

II.TAGUCHIAPPROACH

becoming more widespread in industrial practice. The

application of statistical methods, in particular the design of

experiments, has had considerable impact. The ideas of a very

successful leading quality consultant in Japan, Dr. Taguchi

have been adopted by many American companies in both

manufacturing

and

scientific

experimental designs developed by taguchi known as

orthogonal arrays, are essentially fractional factorials.

Knowing the quantity of parameters and therefore the

number of levels, the appropriate orthogonal array is

designated.

During

this work we

to seized four

plating

with 3 levels. Supported the on top of parameters and levels,

L27

orthogonal

array

was executed for sturdy experimental style. The target of the

present work is to maximize the small hardness of the

Nickel thin film

coatings.

best module is customized .The higher is best representative

of S/N ratio can be framed as

1

10log(

i

N

n

The scientific approach to quality improvement was

circumstances.

The

have

a

tendency

parameters

of

Taguchi

approach

Meanwhile

the

larger is

1

n

S

 

)

y

2

ij

1

(1)

(1)

Where n is cherishing replication of the experimental work

and y represents the output of experiment. Additionally to

mean effects techniques and ANOVA will be enforced to

see the influence of the method parameters on the

performance characteristic.

Fig 1: Formation of electro deposited coating

2 www.erpublication.org


Engineering research paper

International Journal of Engineering and Technical Research (IJETR)

ISSN: 2321-0869, Volume-3, Issue-4, April 2015

Table I: Parameters and levels

Levels

II

2

3.5

Parameters

Units

I

1

III

4

4.5

A/dm2

A. Current density

B. pH

C. Time of

deposition

D. Temperature of

the bath

2.5

min

30

45

60

oC

30

45

60

IV.RESULTS AND DISCUSSION

A. Assessment of surface morphology

morphological examinations via metallographic procedures.

The pattern of deposition of metallic element particles within

the deposit

was

scanning microscope (JEOL–Field emission SEM, model

TSM-6701F, Japan) at numerous magnifications. From on

top of analysis, it absolutely was originate that the particles

were uniformly distributed in nickel matrix with uniform

grains.

The coated samples were organized for surface

Fig 3: EDX Results of Ni thin film coating

B. Assessment of micro hardness of Ni thin film coating

examined

by

Vickers micro hardness tester (model & maker: SHIMADZU

-TYPE HMV- 1/-2, SHIMADZU Corporation, Japan) with

the

payload of

50 gram

indentation amount. The indented location was targeted with

400X Magnification and also the slider positions were

adjusted to the diagonal lengths of indentation. Finally,

the micro hardness

was

system supported and value was

digital scan out. Micro hardness of

examined with four trials and also the average value was

taken for final documentation.

C. Analysis of S/N ratio

Micro hardness of the coated samples were discovered in

force

for 10

sec.

of

calculated

by

a

taken

from

was

every

sample

control factors. The control factors are the desirable one that

can be controlled and noise factors are undesirable one that

amounts for the variation in response characteristics [15]. The

process optimization based on the taguchi approach is on

ground that the noise factors effect can be reduced if we select

proper control factor levels. Larger S\N ratio denotes a higher

performance, independent of the operation characteristics and

therefore the process can be optimized without removing the

cause for variation and making it robust against the noise

factors [16].The formulae for signal/noise are designed such

the experimentalist can always select the larger factor level

settings

to

optimize

characteristics of an experiment. Therefore, the strategy of

calculating the signal-to-noise ratio depends on whether the

quality representative has smaller-the-best, larger-the-better

or nominal-the-better formulation is chosen.

Taguchi related with two main parameters called noise and

the

standard

Fig 2: Micro structure of Nickel thin film coating through

optical micrographs a.100X; b.250X, SEM micrographs: C.

at 385X ; D. 711X

The

investigate the compositional phases in the coated samples.

Fig 3 displays the EDAX results of composite coating and

approves the existence of nickel elements within the matrix.

The EDAX observations confirm the presence of nickel

elements in the deposition over mild steel substrates.

EDAX

observations

were

accomplished to

In this study, the quality characteristic has

larger-the-best formulation and therefore the equation for

calculating S/N ratio is as follows:

S

N

n

1

n

1

10log(

 

)

y

2

ij

1

i

(2)

3 www.erpublication.org


Engineering research paper

Influence of process parameters on Electrodeposited Nickel thin film coating using Taguchi approach

Where (yij) is the value of the micro hardness for the test in

that trial and (n) is the number of tests in a trial, high

signal-to-noise ratios are always preferred.

Table II: Experimental responses for Nickel Thin film

Coating

Control Parameters

a

b

c

d

Mass of

Deposit

mg

33.2

Micro

Hardness

HV

216

S/N

Ratio

dB

46.68

Expt.

No.

1

1

2.5

30

30

2

1

2.5

60

45

38.5

315

49.96

3

1

2.5

90

60

62.6

399.33

52.02

4

1

3.5

30

45

10.3

231.33

47.28

Fig 4: Mean effect plot for S/N ratios

5

1

3.5

60

60

59.7

340.66

50.64

6

1

3.5

90

30

72.3

474

53.51

7

1

4.5

30

60

39.5

332

50.42

8

1

4.5

60

30

46.8

247

47.85

`9

1

4.5

90

45

53

278.66

48.90

10

2

2.5

30

30

62

293.33

49.34

11

2

2.5

60

45

81.2

378.66

51.56

12

2

2.5

90

60

118.7

641.33

56.14

13

2

3.5

30

45

68.4

354.66

50.99

14

2

3.5

60

60

102.3

454.66

53.15

15

2

3.5

90

30

493.6

492.33

53.84

Fig 5: Mean effect plot for means

The significances of S/N ratio and mean effects response

were displayed in Tables .This Table also include the delta

(∆) which is the difference among the highest S/N ratio and

the lowest S/N ratio values. Ranks for factors are assigned on

the basis of the delta value. The highest delta value is assigned

to rank 1; rank 2 is assigned to next highest delta value and the

rest. Based on ranking positions it was observed that, current

densities has the highest delta value, ranked by 1st position

and identified as the most influencing factor on micro

hardness in the Nickel thin plate electro deposition. The

means response table IV designate the percentage of effects of

parameters on response (micro hardness), and the rank orders

were identical to the rank orders of S/N ratio analysis. In order

to confirm the results of S/N ratio and mean effects studies,

ANOVA approach was employed to identify the significances

of process parameters on response variable.

D. Analysis of variance (ANOVA)

16

2

4.5

30

60

60

277.5

48.86

17

2

4.5

60

30

98.3

277

48.84

18

2

4.5

90

45

130.8

582.66

55.30

19

4

2.5

30

30

217.3

478.66

53.60

20

4

2.5

60

45

180.4

770

57.72

21

4

2.5

90

60

210.3

770.33

57.73

22

4

3.5

30

45

112.9

740

57.38

23

4

3.5

60

60

157.7

683.33

56.69

24

4

3.5

90

30

246

680

56.65

25

4

4.5

30

60

107.4

532.66

54.52

26

4

4.5

60

30

97.8

231.33

47.28

27

4

4.5

90

45

231.7

715.33

57.09

Table III: Mean S/N ratio values of parameters on micro

hardness

Level

A

B

C

D

1

49.70

52.76

51.01

50.85

2

52.01

53.35

51.53

52.91

for significant differences between means. In this study the

ANOVA investigations for experimental response were

performed in ANOVA tool offered in MINITAB 16 software

and the end results were tabulated.

Table V: ANOVA table for micro hardness - conventional

type deposition

source

DF

SS

F

A

2

441616

24.91

B

2

59681

3.37

C

2

160505

9.05

D

2

75712

4.27

Error

18

Total

26

The intention of analysis of variance (ANOVA) is to test

3

55.41

51.01

54.58

53.36

DELTA

5.71

2.34

3.57

2.51

RANK

1

4

2

3

Table IV: Mean effects of parameters on micro hardness

Level

A

B

C

D

1

314.9

473.6

384

376.6

p

ρ %

49.23

6.65

17.89

8.44

Rank

1

4

2

3

2

416.9

494.6

410.8

485.1

0.000

0.057

0.002

0.030

159574

897088

3

622.4

386

559.3

492.4

DELTA

% of effect of

parameters

RANK

307.5

108.5

175.3

24.79

%

2

115.8

43.4 %

15.3 %

16.3%

1

4

3

4 www.erpublication.org


Engineering research paper

International Journal of Engineering and Technical Research (IJETR)

ISSN: 2321-0869, Volume-3, Issue-4, April 2015

[4] Zengwei Zhu, Di Zhu, Ningsong Qu, Weining Lei., Electrodeposition of

bright nickel coating under perturbation of hard particles. Materials and

Design, vol. 28, 1776–1779, 2007.

Table V shows the contribution levels (ρ %) of

parameters on micro hardness investigated from ANOVA

module for Ni thin film coating electro deposition. It was

witnessed that, the contributions of parameters on micro

hardness was about current density, (ρ=49.23%); time of

deposition, (ρ=17.89%); temperature of the bath, (ρ=8.44%);

pH of the bath,(6.65%).The above rank orders are worthy

agreed with the rank orders of S-N ratio and mean effect

studies. Thus, the influences and significances of process

parameters on micro hardness of coating confirmed with three

different schemes and authenticated.

[5] A. Godona, J. Creusa, X. Feaugasa, E. Confortob, L. Pichonc, C.

Armandd, C. Savalla., Characterization of electrodeposited nickel

coatings from sulphamate electrolyte without additive. Materials

characterization, vol. 62, pp. 164-173, 2011.

[6] ZHOU Li-qun, LI Yu-ping, ZHOU Yi-chun, Forming limits of nickel

coating on right region. Trans. Nonferrous Met. SOC, China vol. 17, pp.

913-918, 2007.

[7] A. Ul-Hamid, Abdul Quddus, F.K. Al-Yousef, A.I. Mohammed, H.

Saricimen, L.M. Al-Hadhrami., Microstructure and surface mechanical

properties of electrodeposited Ni coating on Al 2014 alloy. Surface &

Coatings Technology, vol. 205, pp. 2023–2030, 2010.

V.CONCLUSIONS

[8] Anette A. Rasmussen, Per Møller, Marcel A.J. Somers , Microstructure

and thermal stability of nickel layers electrodeposited from an

additive-free sulphamate-based electrolyte. Surface & Coatings

Technology, vol. 200, pp. 6037–6046, 2006.

Electrodeposited Nickel thin film coating have been produced

from watts bath. Robust experimental design methodology

has been implemented for effect studies for above depositions

using Taguchi approach with the objective of less

experimental trails and cost effective experimentation. The

following conclusions were established from the experimental

and analytical studies.

L27 orthogonal array of taguchi’s approach was

engaged to frame the experimental trails with least

number of experiments. The experiments were

accomplished by adjusting the process parameters

and levels based on the run orders.

The surface morphological studies for Ni thin film

coating was implemented using optical micrographs

and SEM analysis.

Experimental results such as mass of deposit, coating

thickness, and micro hardness of coating were

examined methodically.

The effects of process parameters on the response

micro hardness were examined via analytical studies

such as mean effect studies and S/N ratio analysis. In

order to confirm the end results of above analysis,

significance analysis studies were conducted using

statistical tool called ANOVA. The significances of

process parameters were ranked by order.

From the above investigations, current density and

time of deposition are the most significance factor

for the hardness for Ni thin film coating;

It is important to note that the mass of deposit was

accomplished from 70.6 to 250.2 mg. The micro

hardness of Ni thin film coating was attained in the

span of 216 to 770.33 HV.

REFERENCES

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Analysis of the composite and film hardness of electrodeposited nickel

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[15]D. Besterfield, C. Besterfield-Michna, G. H. Besterfield.,

M.Besterfield-Sacre, H. Urdhwareshe,R. Urdhwarshe: Total quality

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[16]P. J. Ross, Taguchi techniques for quality engineering (2nd edition),

McGraw-Hill International Editions 1996.

S.Jeyaraj, Assistant Professor, School of MechanicalEngineering,

SASTRA University, Tamil nadu , India. His research interest is

electrodeposited composite coatings and its effects studies.

G.Muralidharan, PG scholar, School of Mechanical Engineering,

SASTRA University, Tamil nadu, India.

K.P. Arulshri, Professor and Head, department of Mechatronics, Bannari

Amman Institute of technology, Tamil nadu, India.His research interest is

Finite element analysis, optimization techniques and material design. He has

published numerous research papers in international journals.

R.Saravanan, PG scholar, School of Mechanical Engineering, SASTRA

University, Tamil nadu, India.

[2] Haijun Zhao, Lei Liu, Jianhua Zhu, Yiping Tang, Wenbin Hu,

Microstructure and corrosion behavior of electrodeposited nickel

prepared from a sulphamate bath, Materials Letters, vol. 61, pp.

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[3] Arman Zarebidaki, Hassan Mahmoudikohani, Mohammad-Reza

Aboutalebi., Microstructure and corrosion behavior of electrodeposited

nano-crystalline nickel coating on AZ91 Mg alloy.

Journal of Alloys and Compounds, vol. 615, pp. 825–830, (2014)

5 www.erpublication.org


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